US4976943A - Spherical, hydrophilic silica, method of its preparation and use - Google Patents

Spherical, hydrophilic silica, method of its preparation and use Download PDF

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Publication number
US4976943A
US4976943A US07/351,054 US35105489A US4976943A US 4976943 A US4976943 A US 4976943A US 35105489 A US35105489 A US 35105489A US 4976943 A US4976943 A US 4976943A
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United States
Prior art keywords
temperature
heated
spherical
tube
hydrophilic silica
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Expired - Fee Related
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US07/351,054
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English (en)
Inventor
Ingo Pauli
Peter Kleinschmit
Rudolf Schwarz
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Evonik Operations GmbH
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Degussa GmbH
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Assigned to DEGUSSA AKTIENGESELLSCHAFT reassignment DEGUSSA AKTIENGESELLSCHAFT ASSIGNMENT OF ASSIGNORS INTEREST. Assignors: KLEINSCHMIT, PETER, PAULI, INGO, SCHWARZ, RUDOLF
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
    • C01B33/181—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process
    • C01B33/183—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process by oxidation or hydrolysis in the vapour phase of silicon compounds such as halides, trichlorosilane, monosilane
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/02—Amorphous compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/32—Spheres
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/51—Particles with a specific particle size distribution
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/90—Other properties not specified above

Definitions

  • the present invention relates to a spherical, hydrophilic silica, the method of its preparation as well as its use.
  • the silica powder prepared according to the state of the art has the disadvantage that it is too fine for the intended usage.
  • a feature of the present invention resides in spherical, hydrophilic silica consisting of compact, massive, non-crystalline particles without inner pores with a particle size of 0.5 to 10 ⁇ m, preferably 0.5 to 4 ⁇ m and especially 1 to 3 ⁇ m with a BET surface area of ⁇ 50 m 2 /g preferably of 1 to 10 m 2 /g.
  • the spherical, hydrophilic silica of the present invention can be used with advantage as filler in electronic packages or as anti-blocking agent in plastic sheets or foils.
  • Further subject matter of the invention is constituted by a method of preparing the spherical, hydrophilic silica consisting of compact, massive, non-crystalline particles without inner pores with a particle size distribution of 0.5 to 10 ⁇ m, preferably 0.5 to 4 ⁇ m and especially 1 to 3 ⁇ m, with a BET surface area of ⁇ 50 m 2 /g, preferably of 1 to 10 m 2 /g.
  • the method is characterized in that two components; namely, water vapor and gaseous silicon tetrachloride, are heated separately to a temperature of 300° to 400° C., the two aforesaid components are then mixed at a temperature of 300° to 400° C.
  • the resulting gaseous mixture is conducted through a narrow prereaction tube heated to a temperature of 600° to 1200° C., then through a wider reaction tube heated to 600° to 1000° C., preferably 700° to 800° C., with a dwell time of >5 sec., preferably >9 sec. and with a vacuum of at least 100 mm H 2 O column and the reaction product is separated from the reaction gases.
  • the silica of the invention can be used with a high degree of filling of 60% in resins used to manufacture electronic packages.
  • Such a capsule for integrated circuits can be formed of an epoxy low-pressure moulding material.
  • the silica of the intention has the advantage that a degassing of the resinous moulding material can be carried out without foaming.
  • the tube reactor is heated by external heating to a temperature of 730° C.
  • the dwell time of the two gases in the reactor is 9.53 sec.
  • a vacuum of 100 mm H 2 O column is maintained in the reactor.
  • the silicon dioxide obtained exhibits a particle size distribution of 0.5 to 4 ⁇ according to REM and TEM.
  • the specific surface area is 2.3 m 2 /g.
  • Gaseous silicon tetrachloride and water are obtained and mixed in a molar ratio of 1:6.81 at 100°-400° C.
  • the mixture is passed through a conventional prereaction tube heated to 800° C. These gaseous components are subsequently reacted with one another at 700° ⁇ 20° C.
  • the silicon dioxide obtained exhibits a particle size distribution according to FIG. 1, determined with a Cilas-Alcatel Granulometer HR 850 163.
  • the average particle size is 1.86 ⁇ m.
  • the BET surface area is 3.1 m 2 /g (DIN 66 131).
  • German priority application No. P 38 17 045.0-41 is relied on and incorporated herein.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
US07/351,054 1988-05-19 1989-05-12 Spherical, hydrophilic silica, method of its preparation and use Expired - Fee Related US4976943A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3817045 1988-05-19
DE3817045 1988-05-19

Publications (1)

Publication Number Publication Date
US4976943A true US4976943A (en) 1990-12-11

Family

ID=6354684

Family Applications (1)

Application Number Title Priority Date Filing Date
US07/351,054 Expired - Fee Related US4976943A (en) 1988-05-19 1989-05-12 Spherical, hydrophilic silica, method of its preparation and use

Country Status (4)

Country Link
US (1) US4976943A (ko)
JP (1) JPH0238306A (ko)
KR (1) KR910004832B1 (ko)
BR (1) BR8902288A (ko)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6672110B2 (en) 1998-12-17 2004-01-06 Pirelli Cavi E Sistemi S.P.A. Method of forming an optical fiber preform by combustionless hydrolysis
US20130045439A1 (en) * 2011-08-18 2013-02-21 Shin-Etsu Chemical Co., Ltd. Titania-doped quartz glass and making method

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE13400C (de) * R. SCHNEIDER in Düsseldorf Neuerungen an dem durch Patent 108866 geschützten Mahlwerk mit konoidischem Läufer
DE973859C (de) * 1951-10-31 1960-06-30 Dow Corning Verfahren zur Herstellung feinverteilter hydrophober Kieselsaeure
CA662036A (en) * 1963-04-30 L. Flemmert Gosta Production of hydrophilic silicon dioxide

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01145317A (ja) * 1987-12-01 1989-06-07 Nippon Shokubai Kagaku Kogyo Co Ltd 真球状シリカ微粒子の製法

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE13400C (de) * R. SCHNEIDER in Düsseldorf Neuerungen an dem durch Patent 108866 geschützten Mahlwerk mit konoidischem Läufer
CA662036A (en) * 1963-04-30 L. Flemmert Gosta Production of hydrophilic silicon dioxide
DE973859C (de) * 1951-10-31 1960-06-30 Dow Corning Verfahren zur Herstellung feinverteilter hydrophober Kieselsaeure

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6672110B2 (en) 1998-12-17 2004-01-06 Pirelli Cavi E Sistemi S.P.A. Method of forming an optical fiber preform by combustionless hydrolysis
US20130045439A1 (en) * 2011-08-18 2013-02-21 Shin-Etsu Chemical Co., Ltd. Titania-doped quartz glass and making method
US9346700B2 (en) * 2011-08-18 2016-05-24 Shin-Etsu Chemical Co., Ltd. Titania-doped quartz glass and making method

Also Published As

Publication number Publication date
JPH0563409B2 (ko) 1993-09-10
JPH0238306A (ja) 1990-02-07
KR900017909A (ko) 1990-12-20
BR8902288A (pt) 1990-01-09
KR910004832B1 (ko) 1991-07-13

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